KR20000049192A - Urea grease composition - Google Patents

Urea grease composition Download PDF

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KR20000049192A
KR20000049192A KR1019990703290A KR19997003290A KR20000049192A KR 20000049192 A KR20000049192 A KR 20000049192A KR 1019990703290 A KR1019990703290 A KR 1019990703290A KR 19997003290 A KR19997003290 A KR 19997003290A KR 20000049192 A KR20000049192 A KR 20000049192A
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urea
grease
urea grease
grease composition
weight
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KR1019990703290A
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KR100503107B1 (en
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마스모리류이찌
오자끼다까히로
무나까따도모오
요시다쓰또무
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지스트라텐 알베르터스 빌헬머스 요안느
쉘 인터내셔날 리서치 마챠피즈 비.브이.
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06—Mixtures of thickeners and additives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M115/00—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
    • C10M115/08—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M119/00—Lubricating compositions characterised by the thickener being a macromolecular compound
    • C10M119/24—Lubricating compositions characterised by the thickener being a macromolecular compound containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/12—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M135/14—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond
    • C10M135/18—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond thiocarbamic type, e.g. containing the groups
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M137/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing phosphorus
    • C10M137/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing phosphorus having no phosphorus-to-carbon bond
    • C10M137/04—Phosphate esters
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/006—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions used as thickening agents
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/026—Amines, e.g. polyalkylene polyamines; Quaternary amines used as thickening agents
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/08—Amides
    • C10M2215/0813—Amides used as thickening agents
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/10—Amides of carbonic or haloformic acids
    • C10M2215/1013—Amides of carbonic or haloformic acids used as thickening agents
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/10—Amides of carbonic or haloformic acids
    • C10M2215/102—Ureas; Semicarbazides; Allophanates
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/10—Amides of carbonic or haloformic acids
    • C10M2215/102—Ureas; Semicarbazides; Allophanates
    • C10M2215/1026—Ureas; Semicarbazides; Allophanates used as thickening material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/12—Partial amides of polycarboxylic acids
    • C10M2215/121—Partial amides of polycarboxylic acids used as thickening agents
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/2206—Heterocyclic nitrogen compounds used as thickening agents
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/225—Heterocyclic nitrogen compounds the rings containing both nitrogen and oxygen
    • C10M2215/227—Phthalocyanines
    • C10M2215/2275—Phthalocyanines used as thickening agents
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/044—Polyamides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/045—Polyureas; Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
    • C10M2219/066—Thiocarbamic type compounds
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    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
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    • C10M2219/068—Thiocarbamate metal salts
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    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
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    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
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    • C10M2223/041—Triaryl phosphates
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    • C10N2010/00—Metal present as such or in compounds
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/06—Instruments or other precision apparatus, e.g. damping fluids

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
  • Fats And Perfumes (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

PURPOSE: An urea grease is provided, which is excellent in frictional properties and wear resistance and also has good fitting property to sealants such as chloroprene rubber and polyester resin. CONSTITUTION: An urea grease composition comprises a urea grease and as additives: (A) a molybdenum dialkyldithiocarbamate sulfide represented by formula (I), wherein R1 and R2 each independently represents a group selected from the group consisting of alkyl groups having from 1 to 24 carbon atoms; m is 0 or an integer of from 1 to 3; and n is an integer of from 1 to 4; the sum of m and n is 4; and (B) a triphenyl phosphate represented by formula (II).

Description

요소 그리스 조성물 {UREA GREASE COMPOSITION}Urea grease composition {UREA GREASE COMPOSITION}

본 발명은 요소 그리스 조성물, 및 상기 조성물을 함유하는 기어에 관한 것이다. 소위 말하는 오일 쇼크로 인해 석유의 비용이 급격하게 증가함으로써, 모든 산업 분야에서는 이의 영향을 반영하듯, 원료 절감 및 에너지 절약에 대한 아이디어가 꾸준히 제기되었다.The present invention relates to a urea grease composition and a gear containing the composition. So-called oil shocks have dramatically increased the cost of petroleum, and the idea of raw material savings and energy savings has been continually raised, reflecting its impact in all industries.

자동차 산업에서는 소형이며 가벼운 대중적인 자동차가 개발되었으며, 일정 속도 조인트 (이하,“CVJ”라 약칭함) 를 사용하는 자동차의 수가 증가하였다. 또한, CVJ 는 4 륜 구동 자동차 및 4 륜 독립 서스펜션 유형의 자동차에 사용되며, 그 수요가 증가하고 있다. 또한 일정 속도 유니버셜 조인트라고도 불리는 CVJ 는 일정한 각속도 및 토오크를 유지하는 회전을 전달하는 조인트로서, 각종 용도에 따라 여러가지 형태를 가진다. CVJ 에 사용되는 윤활제는 자동차가 고동력 및 고속력에 이르게 됨에 따라 보다 심각한 상황에 노출되며 CVJ 자체는 압축되기 때문에, 슬라이딩 부분에 대한 마찰 및 마모를 줄이기 위해 그리스가 요구된다. 또한, 그리스의 누출과 외부로부터의 이물질 및 물의 침입을 막기 위해서, CVJ 상에 시일 부트 멤버를 설치하는 것이 요구된다. 이러한 물질로는, 통상 클로로프렌 고무가 사용되며, 또한 일반적으로 폴리에스테르 수지가 사용된다.In the automotive industry, compact and lightweight popular cars have been developed, and the number of cars using constant speed joints (abbreviated as “CVJ”) has increased. In addition, CVJ is used in four-wheel drive cars and four-wheel independent suspension type cars, the demand is increasing. CVJ, also called constant velocity universal joint, is a joint that transmits rotation to maintain a constant angular velocity and torque, and has various forms according to various applications. Lubricants used in the CVJ are exposed to more serious situations as the vehicle reaches high and high speeds, and since the CVJ itself is compressed, grease is required to reduce friction and wear on the sliding parts. In addition, in order to prevent the leakage of grease and the intrusion of foreign matter and water from the outside, it is required to install a seal boot member on the CVJ. As such a material, chloroprene rubber is usually used, and polyester resin is generally used.

저 마찰 및 내마모성이 우수한 그리스는 출발 및 가속시, 또한 구동 동안에 자동차 차체의 진동 및 소음을 억제한다. 더욱이, 온도 억제 효과로 인해, 시일 부트 멤버의 내구성이 향상될 수 있다. 그러나, 온도의 과도한 증가는 시일 부트 멤버의 노화 및 윤활제의 분해를 촉진하고, CVJ 의 수명을 극도로 단축시킨다.Greases with good low friction and wear resistance suppress vibration and noise of the vehicle body at the start and acceleration and also during driving. Moreover, due to the temperature suppressing effect, the durability of the seal boot member can be improved. However, excessive increase in temperature promotes aging of the seal boot member and decomposition of the lubricant, and extremely shortens the life of the CVJ.

한편, 철강 산업에서는 또한 기계 설비의 연속 작업이 이루어졌다. 이러한 기술적 대변혁으로, 고 품질의 제품, 제조 능력의 향상, 장치의 신뢰성 보장 등이 강력하게 요구되었다. 이들 기계 장치에 사용되는 그리스는 고온, 물과의 접촉, 찌끼와 같은 이물질의 높은 침입 가능성 등의 곤란한 환경에 놓이며, 밤낮으로 심각한 상황에 노출되기 때문에, 윤활 조건은 매우 엄격하다. 그리스는 기계 부품의 수명을 연장하며 돌연한 파손을 최대한 막기 위해서, 우수한 시일 내성을 가지며 마찰 및 마모를 감소시키는 것이 요구된다. 또한, 공업용 기계, 기계 공구 등의 윤활하고자 하는 부품은 상당한 마찰을 격게되며, 과도한 마모는 기계의 정밀성을 저하시키기 때문에, 기계 부품을 교체해야만 한다. 상술한 바와 같이, 마찰 감소 및 마모 저하는 본 발명의 중요한 목적이다.On the other hand, the steel industry also had a continuous operation of machinery. With this technological revolution, there has been a strong demand for high quality products, improved manufacturing capability, and reliability of devices. Greases used in these machinery are subjected to difficult environments, such as high temperatures, contact with water, high potential for ingress of foreign matter such as tailings, and are exposed to severe conditions day and night, so lubrication conditions are very strict. Grease is required to have good seal resistance and to reduce friction and wear, in order to extend the life of mechanical parts and to prevent sudden breakage as much as possible. In addition, parts to be lubricated, such as industrial machines, machine tools, and the like, are subjected to considerable friction, and excessive wear deteriorates the precision of the machine, and therefore, mechanical parts must be replaced. As mentioned above, friction reduction and wear reduction are important objects of the present invention.

그러므로, 상술한 바와 같은 윤활하고자 하는 부품에서는, 황화 지방 및 오일, 황화 올레핀 등과 같은 황-기재 화합물, 납 나프테네이트, 금속 디티오포스페이트, 금속 디티오카르바메이트-기재 첨가제 등을 이용하여, 리튬-기재 그리스가 편리하게 사용되었다. 최근에는, 리튬-기재 그리스 보다 내열성이 뛰어난 리튬 착물 그리스 및 요소 그리스의 사용이 급증하였다.Therefore, in the parts to be lubricated as described above, using sulfur-based compounds such as sulfurized fats and oils, sulfide olefins, lead naphthenates, metal dithiophosphates, metal dithiocarbamate-based additives, and the like, Lithium-based greases were conveniently used. In recent years, the use of lithium complex grease and urea grease which is more excellent in heat resistance than lithium-based grease has increased rapidly.

이러한 상황하에서, 전형적인 종래 기술의 하나로서, 미국 특허 제 4,514,312 호에는 요소 그리스내에 황을 함유하지 않으며, 유기 첨가제로서 방향족 아민 포스페이트를 사용하는 그리스가 개시되어 있다. 또한, 미국 특허 제 4,840,740 호에는 요소 그리스, 유기 몰리브덴 화합물 및 아연 디티오포스페이트를 포함하는 그리스가 개시되어 있다. 일본 특허 공보 (JP-B) 제 04-34590 (1992) 호에는 (1) 몰리브덴 디알킬디티오카르바메이트 설파이드 및 (2) 황화 지방 및 오일, 황화 올레핀, 트리크레실 포스페이트, 트리알킬 티오포스페이트 및 아연 디알킬 디티오포스페이트로 구성되는 군에서 선택되는 1 종, 또는 이들의 2 종 이상의 조합체를 포함하는 황-인-기재의 초고압 첨가제를 필수 성분으로서 함유하는 요소 그리스가 개시되어 있다.Under these circumstances, as one of the typical prior art, US Pat. No. 4,514,312 discloses a grease that does not contain sulfur in urea grease and uses aromatic amine phosphate as an organic additive. In addition, US Pat. No. 4,840,740 discloses a grease comprising urea grease, an organic molybdenum compound, and zinc dithiophosphate. Japanese Patent Publication (JP-B) No. 04-34590 (1992) includes (1) molybdenum dialkyldithiocarbamate sulfides and (2) sulfided fats and oils, sulfided olefins, tricresyl phosphates, trialkyl thiophosphates And urea grease containing as an essential component a sulfur-phosphorus-based ultrahigh pressure additive comprising one or a combination of two or more thereof selected from the group consisting of zinc dialkyl dithiophosphates.

종래 기술의 그리스의 일부가 마찰 및 마모 감소 효과를 갖는 것으로 알려져 있으나, 완전히 만족할 정도는 아니다. 또한, 실런트가 고온에서 열화되는 단점이 있다. 예를 들면, 방향족 아민 포스페이트 및 납 나프테네이트는 폴리에스테르 수지를 분해시키고, 황화 지방 및 오일은 클로로프렌 고무를 분해시키며, 황화 올레핀은 클로로프렌 고무와 폴리에스테르 수지 모두를 상당히 분해시킨다.Some of the prior art greases are known to have friction and wear reduction effects, but are not completely satisfactory. In addition, there is a disadvantage that the sealant deteriorates at a high temperature. For example, aromatic amine phosphates and lead naphthenates degrade polyester resins, sulfided fats and oils degrade chloroprene rubbers, and sulfide olefins significantly degrade both chloroprene rubbers and polyester resins.

또한, 다른 종래 기술로서, 일본 특허 출원 공개 (JP-A) 제 08-157859 호 (1996) 에서는 첨가제로서 몰리브덴 디알킬디티오카르바메이트 설파이드 및 트리페닐포스포로티오네이트를 사용하고 있고, 일본 특허 출원 공개 (JP-A) 제 62-2275197 호 (1987) 에서는 증점제로서 12-히드록시 지방산의 리튬 비누, 트리메틸 포스페이트 또는 트리페닐 포스페이트와 같은 포스페이트로부터 형성된 리튬 포스페이트를 사용하고 있다. 또한, 일본 특허 출원 공개 (JP-A) 제 03-231993 호 (1991) 에는 요소 화합물에 포스페이트 오일을 사용하는 그리스 조성물이 개시되어 있다.As another conventional technique, Japanese Patent Application Laid-Open (JP-A) No. 08-157859 (1996) uses molybdenum dialkyldithiocarbamate sulfide and triphenylphosphorothionate as additives, and Japanese Patent Application Application publication (JP-A) 62-2275197 (1987) uses lithium phosphate formed from phosphates such as lithium soap, trimethyl phosphate or triphenyl phosphate of 12-hydroxy fatty acids as thickener. In addition, Japanese Patent Application Laid-Open (JP-A) No. 03-231993 (1991) discloses a grease composition using phosphate oil as a urea compound.

본 발명은 마찰 특성 및 내마모성이 우수하며, 클로로프렌 고무 및 폴리에스테르 수지와 같은 실런트에 대해 양호한 접착성을 갖는 요소 그리스에 관한 것이다. 더욱 구체적으로, 본 발명은 자동차의 일정 속도 조인트, 볼 조인트 및 볼 베어링, 및 강철, 공업용 기계 및 기계 공구와 같은 각종 공업용 장비의 베어링 및 기어와 같은 그리스-윤활하고자 하는 부품에 사용하기 적합한 요소 그리스 조성물에 관한 것이다.The present invention relates to urea grease, which is excellent in friction properties and abrasion resistance, and has good adhesion to sealants such as chloroprene rubber and polyester resin. More specifically, the present invention provides element greases suitable for use in grease-lubricated parts such as constant speed joints, ball joints and ball bearings of automobiles, and bearings and gears of various industrial equipment such as steel, industrial machines and machine tools. It relates to a composition.

본 발명은 요소 그리스, 및 첨가제로서 (A) 하기 화학식 I 로 표시되는 몰리브덴 디알킬디티오카르바메이트 설파이드 및 (B) 하기 화학식 II 로 표시되는 트리페닐 포스페이트를 포함하는 요소 그리스 조성물에 관한 것이다 :The present invention relates to a urea grease composition comprising urea grease and (A) molybdenum dialkyldithiocarbamate sulfide represented by formula (I) and triphenyl phosphate represented by formula (II):

(식중, R1및 R2는 각각 독립적으로 C1-24알킬기로 구성되는 군에서 선택되는 기이고, m 은 0 또는 1 내지 3 의 정수이며, n 은 1 내지 4 의 정수이되, 단 m+n 은 4 이다)(Wherein R 1 and R 2 are each independently a group selected from the group consisting of C 1-24 alkyl groups, m is 0 or an integer of 1 to 3, n is an integer of 1 to 4, provided that m + n is 4)

상기 성분 (A) 에 상응하는 화합물은 고 융점을 가진다. 이들 화합물의 예로는 디에틸 설파이드-몰리브덴 디티오카르바메이트, 디부틸-몰리브덴 디티오카르바메이트, 디이소부틸 설파이드-몰리브덴 디티오카르바메이트, 디(2-에틸헥실)설파이드-몰리브덴 디티오카르바메이트, 디아밀 설파이드-몰리브덴 디티오카르바메이트, 디이소아밀 설파이드-몰리브덴 디티오카르바메이트, 디라우릴 설파이드-몰리브덴 디티오카르바메이트, 디스테아릴 설파이드-몰리브덴 디티오카르바메이트가 있다. 이들은 바람직하게는 분말 형태로 혼합되며, 첨가량은 상기 조성물의 총중량에 대해서 0.5 내지 10 중량%, 바람직하게는 0.5 내지 5 중량% 이다. 상기 첨가량이 0.5 중량% 이하인 경우에는 내마찰성 및 내마모성의 향상 효과가 불충분하며, 10 중량% 이상인 경우에는 추가의 향상이 일어나지 않는다.The compound corresponding to component (A) has a high melting point. Examples of these compounds include diethyl sulfide-molybdenum dithiocarbamate, dibutyl-molybdenum dithiocarbamate, diisobutyl sulfide-molybdenum dithiocarbamate, di (2-ethylhexyl) sulfide-molybdenum dithio Carbamate, diamyl sulfide-molybdenum dithiocarbamate, diisoamyl sulfide-molybdenum dithiocarbamate, dilauryl sulfide-molybdenum dithiocarbamate, distearyl sulfide-molybdenum dithiocarbamate have. They are preferably mixed in powder form and the amount added is 0.5 to 10% by weight, preferably 0.5 to 5% by weight, relative to the total weight of the composition. If the added amount is 0.5% by weight or less, the effect of improving friction resistance and abrasion resistance is insufficient, and when it is 10% by weight or more, no further improvement occurs.

상기 트리페닐 포스페이트는 융점이 50 ℃ 이고 주위 온도에서 고체이며, 상기 분말은 베이스 그리스와 50 ℃ 이상의 온도에서 혼합한다. 상기 성분 (B) 의 양은 상기 조성물의 총중량에 대해서 바람직하게는 0.1 내지 10 중량% 이고, 더욱 바람직하게는 0.1 내지 5 중량% 이다. 상기 사용량이 0.1 중량% 이하인 경우에는 내마찰성 및 내마모성의 향상을 달성할 수 없으며, 10 중량% 이상인 경우에는 추가의 윤활력을 수득할 수 없다.The triphenyl phosphate has a melting point of 50 ° C. and a solid at ambient temperature, and the powder is mixed with the base grease at a temperature of 50 ° C. or higher. The amount of the component (B) is preferably 0.1 to 10% by weight, more preferably 0.1 to 5% by weight relative to the total weight of the composition. When the amount used is 0.1% by weight or less, the improvement of the friction resistance and the wear resistance cannot be achieved, and when the amount is 10% by weight or more, additional lubricating power cannot be obtained.

요소 화합물로는, 요소 유형의 공지의 임의의 증점제를 사용할 수 있다. 예를 들면, 이요소 (diurea), 삼요소 (triurea) 및 사요소 (tetraurea) 를 사용할 수 있다.As the urea compound, any known thickener of urea type can be used. For example, diurea, triurea and tetraurea can be used.

베이스 오일로는, 광유 및/또는 합성유를 사용할 수 있다. 요소 화합물을 증점제로서 사용하는 경우에는, 상기 베이스 오일과 요소 화합물의 총중량에 대해서 2 내지 35 중량% 의 양으로 첨가하는 것이 바람직하다.As the base oil, mineral oil and / or synthetic oil can be used. When using urea compound as a thickener, it is preferable to add in the amount of 2 to 35 weight% with respect to the total weight of the said base oil and urea compound.

또한, 본 발명의 조성물에는 산화방지제, 부식방지제, 초고압제, 중합체 등과 같은 각종 첨가제를 추가로 첨가할 수 있다.In addition, various additives such as antioxidants, corrosion inhibitors, ultrahigh pressure agents, polymers, and the like may be further added to the composition of the present invention.

본 발명에 의한 요소 그리스 조성물은 기어, 더욱 구체적으로는 일정 속도 조인트에 특히 적합하게 사용된다. 그러므로, 본 발명은 또한 상기 그리스를 함유하는 기어, 더욱 구체적으로는 일정 속도 조인트에 관한 것이다.The elemental grease composition according to the invention is particularly suitably used for gears, more particularly for constant velocity joints. The invention therefore also relates to a gear containing said grease, more particularly to a constant velocity joint.

실시예 및 비교예Examples and Comparative Examples

다음에, 하기의 실시예 및 비교예에 의거하여 본 발명을 상세하게 설명하고자 한다. 그러나, 본 발명은 이들 실시예로 한정되는 것은 아니다.Next, the present invention will be described in detail based on the following Examples and Comparative Examples. However, the present invention is not limited to these examples.

첨가제를 하기 표 1 내지 5 에 제시한 혼합비로 베이스 그리스에 첨가하고 (이들은 모두 중량% 로 나타냄), 그 혼합물을 3-롤 밀로 처리하여 실시예 및 비교예의 그리스를 수득하였다.Additives were added to the base grease at the mixing ratios set forth in Tables 1 to 5 below (all of which are expressed in weight percent) and the mixture was treated with a 3-roll mill to obtain the greases of the examples and comparative examples.

후술하는 바와 같이 베이스 그리스를 제조하였다. 베이스 오일로는, 100 ℃ 에서 15 ㎟/초의 속도를 갖는 정제 광유를 사용하였다.Base grease was prepared as described below. As the base oil, refined mineral oil having a speed of 15 mm 2 / sec at 100 ° C was used.

I. 이요소 (diurea) 그리스I. Diurea Grease

디페닐메탄-4,4'-디이소시아네이트 1 몰과 옥틸아민 2 몰을 베이스 오일중에서 반응시키고, 생성된 요소 화합물을 균일하게 분산시켜 그리스를 수득하였다. 요소 화합물의 양은 베이스 오일과 요소 화합물의 총중량에 대해서 10 중량% 였다.One mole of diphenylmethane-4,4'-diisocyanate and two moles of octylamine were reacted in the base oil, and the resulting urea compound was uniformly dispersed to obtain grease. The amount of urea compound was 10% by weight relative to the total weight of the base oil and the urea compound.

II. 사요소 (tetraurea) 그리스II. Tetraurea Greece

디페닐메탄-4,4'-디이소시아네이트 2 몰, 옥틸아민 2 몰 및 에틸렌디아민 1 몰을 베이스 오일중에서 반응시키고, 생성된 요소 화합물을 균일하게 분산시켜 그리스를 수득하였다. 요소 화합물의 양은 베이스 오일과 요소 화합물의 총중량에 대해서 15 중량% 였다.2 moles of diphenylmethane-4,4'-diisocyanate, 2 moles of octylamine and 1 mole of ethylenediamine were reacted in the base oil, and the resulting urea compound was dispersed uniformly to obtain grease. The amount of urea compound was 15% by weight relative to the total weight of the base oil and the urea compound.

III. 리튬 착물 그리스III. Lithium complex grease

수소화 카스테르 오일 지방산을 베이스 오일에 용해시키고, 중화를 위해 수산화리튬 수용액을 첨가한 후, 그 혼합물을 반응 동안에 탈수시켰다. 탈수를 완료한 후, 아젤라산을 첨가하였다. 중화에 필요한 양의 수산화리튬 수용액으로 반응을 수행하였다. 리튬 아젤레이트와 리튬 12-히드록시스테아레이트 비누를 혼합하고 균일하게 분산시켜 그리스를 수득하였다. 증점제로서 리튬 12-히드록시스테아레이트의 양 및 리튬 아젤레이트의 양은 베이스 오일과 증점제의 총중량에 대해서 각각 7.5 중량% 및 2.5 중량% 였다.The hydrogenated castor oil fatty acid was dissolved in the base oil and an aqueous lithium hydroxide solution was added for neutralization, and then the mixture was dehydrated during the reaction. After dehydration was complete, azelaic acid was added. The reaction was carried out with an aqueous lithium hydroxide solution in an amount necessary for neutralization. Lithium azelate and lithium 12-hydroxystearate soap were mixed and uniformly dispersed to obtain grease. The amounts of lithium 12-hydroxystearate and lithium azelate as thickeners were 7.5% and 2.5% by weight, respectively, relative to the total weight of the base oil and the thickener.

하기 표에 제시한 마찰 계수, 내마모성 및 실런트에 대한 접착성에 대하여 하기의 시험을 수행하였으며, 이들을 평가하였다.The following tests were carried out for the coefficient of friction, abrasion resistance and sealant shown in the following table, and these were evaluated.

(1) 마찰 계수(1) friction coefficient

Falex 시험 기기를 사용하여, 하기의 조건하에서 15 분후의 마찰 계수를 측정하였다 (IP/241/69 에 따름).Using a Falex test instrument, the friction coefficient after 15 minutes was measured under the following conditions (according to IP / 241/69).

회전 속도 : 290 rpmRotational Speed: 290 rpm

하중 : 890 N (200 lb)Load: 890 N (200 lb)

온도 : 실온Temperature: room temperature

시간 : 15 분Time: 15 minutes

그리스의 양 : 시험편에 약 1 g 의 그리스를 도포함Grease Amount: Include approximately 1 g of grease in the specimen.

(2) 내마모성(2) wear resistance

ASTM D2226 의 4-볼 유형 마모 시험에 따름According to ASTM D2226, 4-ball type wear test

회전 속도 : 1200 rpmRotational Speed: 1200 rpm

하중 : 392 N (40 ㎏f)Load: 392 N (40 kgf)

온도 : 75 ℃Temperature: 75 ℃

시간 : 60 분Time: 60 minutes

(3) 실런트에 대한 접착성(3) adhesion to sealant

폴리에스테르 수지 및 클로로프렌 고무로 된 실런트를 각각의 그리스 조성물에 침지시키고, JIS K6301 의 가황 고무 물리적 시험에 따라, 하기 조건하에서 시험하였다. 상기 시험 전 및 후의 인장 강도 및 신율을 측정하였으며, 변화 (%) 를 수득하였다.Sealants made of polyester resin and chloroprene rubber were immersed in the respective grease compositions, and tested under the following conditions in accordance with the vulcanized rubber physical test of JIS K6301. Tensile strength and elongation before and after the test were measured and a change (%) was obtained.

온도 : 140 ℃Temperature: 140 ℃

침지 시간 : 96 시간Immersion time: 96 hours

실시예 1 내지 7 의 마찰 계수는 비교예 1 내지 10 에 비하여 모두 작았다. 내마모성에 관하여, 비교예 5, 6, 7, 9 및 10 은 본 발명의 실시예와 동일한 정도의 양호한 결과를 제공한다. 그러나, 이들 비교예는 클로로프렌 고무 및/또는 폴리에스테르 수지와의 상용성이 불량하다.The friction coefficients of Examples 1 to 7 were all smaller than those of Comparative Examples 1 to 10. With regard to the wear resistance, Comparative Examples 5, 6, 7, 9 and 10 give the same good results as the examples of the present invention. However, these comparative examples are poor in compatibility with chloroprene rubber and / or polyester resin.

예를 들면, 비교예 5 에서는 클로로프렌 고무 및 폴리에스테르 수지의 신율 변화가 크다. 비교예 6 에서는 클로로프렌 고무 및 폴리에스테르 수지의 인장 강도 및 신율 변화가 크다. 비교예 9 및 10 에서는 폴리에스테르 수지의 신율 변화가 비교적 크다. 실시예 1 내지 7 은 우수한 마찰 계수 및 내마모성, 및 또한 클로로프렌 고무 및 폴리에스테르 수지로 된 실런트에 대한 우수한 접착성을 제공한다.For example, in the comparative example 5, elongation change of chloroprene rubber and polyester resin is large. In Comparative Example 6, changes in tensile strength and elongation of chloroprene rubber and polyester resin are large. In Comparative Examples 9 and 10, the elongation change of the polyester resin is relatively large. Examples 1 to 7 provide excellent coefficient of friction and wear resistance, and also good adhesion to sealants made of chloroprene rubber and polyester resin.

본 발명의 그리스는 낮은 마찰 계수와 우수한 내마모성을 가진다. 그 결과, 자동차의 CVJ 의 진동 및 소음이 억제된다. 또한, 본 발명의 그리스는 자동차의 볼 조인트 및 휠 베어링, 및 기타 각종 공업용 기계 장치의 마찰을 감소시키며, 기계 부품의 수명을 연장시킬 수 있다.The grease of the present invention has a low coefficient of friction and good wear resistance. As a result, vibration and noise of the CVJ of the automobile are suppressed. In addition, the grease of the present invention can reduce the friction of ball joints and wheel bearings of automobiles, and other various industrial mechanical devices, and can extend the life of mechanical parts.

본 발명의 그리스는 클로로프렌 고무 및 폴리에스테르 수지에 대한 접착성이 우수하며, 고온에서 조차도 실링된 장치의 실런트의 분해를 지연시킨다.The grease of the present invention is excellent in adhesion to chloroprene rubber and polyester resins and retards decomposition of the sealant of the sealed device even at high temperatures.

Claims (5)

요소 그리스, 및 첨가제로서 (A) 하기 화학식 I 로 표시되는 몰리브덴 디알킬디티오카르바메이트 설파이드 및 (B) 하기 화학식 II 로 표시되는 트리페닐 포스페이트를 포함하는 요소 그리스 조성물 :Urea grease composition comprising urea grease and (A) molybdenum dialkyldithiocarbamate sulfide represented by formula (I) and triphenyl phosphate represented by formula (II): [화학식 I][Formula I] (식중, R1및 R2는 각각 독립적으로 C1-24알킬기로 구성되는 군에서 선택되는 기이고, m 은 0 또는 1 내지 3 의 정수이며, n 은 1 내지 4 의 정수이되, 단 m+n 은 4 이다)(Wherein R 1 and R 2 are each independently a group selected from the group consisting of C 1-24 alkyl groups, m is 0 or an integer of 1 to 3, n is an integer of 1 to 4, provided that m + n is 4) [화학식 II][Formula II] 제 1 항에 있어서, 상기 성분 (A) 및 성분 (B) 가 상기 요소 그리스 조성물의 총중량에 대해서 각각 0.5 내지 10 중량% 및 0.1 내지 10 중량% 의 양으로 혼합되는 요소 그리스 조성물.The urea grease composition according to claim 1, wherein the component (A) and the component (B) are mixed in amounts of 0.5 to 10% by weight and 0.1 to 10% by weight, respectively, relative to the total weight of the urea grease composition. 제 1 항 또는 제 2 항에 있어서, 상기 요소 그리스가 베이스 오일 및 증점제로서 요소 화합물을 포함하고, 상기 요소 화합물의 비율은 상기 베이스 오일과 요소 화합물의 총중량에 대해서 2 내지 35 중량% 인 요소 그리스 조성물.The urea grease composition according to claim 1 or 2, wherein the urea grease comprises a urea compound as a base oil and a thickener, and the ratio of the urea compound is 2 to 35% by weight relative to the total weight of the base oil and the urea compound. . 제 1 항 내지 제 3 항중 어느 한 항에 의한 요소 그리스 조성물을 함유하는 기어.A gear containing the urea grease composition according to any one of claims 1 to 3. 제 4 항에 있어서, 기어가 일정 속도 조인트인 기어.The gear of claim 4 wherein the gear is a constant speed joint.
KR10-1999-7003290A 1996-10-18 1997-10-17 Urea grease composition KR100503107B1 (en)

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JP2004059604A (en) * 2002-07-24 2004-02-26 Nippon Oil Corp Grease composition
CN1292060C (en) * 2002-08-21 2006-12-27 西铁城钟表株式会社 Grease composition for precision equipment and timepiece containing the same
JP2005008744A (en) 2003-06-18 2005-01-13 Showa Shell Sekiyu Kk Grease composition
JP2005248034A (en) * 2004-03-04 2005-09-15 Ntn Corp Grease composition, its preparation method, and antifriction bearing filled with the grease composition
JP4776193B2 (en) * 2004-09-07 2011-09-21 Ｎｔｎ株式会社 Grease composition for automobile wheel bearing
JP4809603B2 (en) 2004-11-25 2011-11-09 本田技研工業株式会社 Constant velocity joint
JP4461000B2 (en) * 2004-11-25 2010-05-12 本田技研工業株式会社 Grease composition for constant velocity joint and constant velocity joint
JP5335019B2 (en) * 2011-03-07 2013-11-06 Ｎｔｎ株式会社 Grease composition for automobile wheel bearing
JP5826626B2 (en) 2011-12-22 2015-12-02 昭和シェル石油株式会社 Grease composition
JP6292569B2 (en) * 2013-12-04 2018-03-14 協同油脂株式会社 Grease composition for constant velocity joint and constant velocity joint enclosing the grease composition
CN104164286A (en) * 2014-08-05 2014-11-26 中国石油化工股份有限公司 Lubricating grease composition for steering ball joint and preparation method of lubricating grease composition

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